反应详情

To a suspension of 1.0 g of 3-iodo-1-trityl-1H-pyrazolo[3,4-c]pyridine-5-carboxylic acid in tert-butanol were added 0.57 g of diphenylphosphoryl azide and 0.31 mL of triethylamine at room temperature, and heated at reflux for 6 hours. The solution was diluted with ethyl acetate, the organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10), to afford 455 mg of the title compound as colorless crystals.

1. temperatureheated
2. temperatureat reflux for 6 hours
3. washthe organic layer was washed successively with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated
6. customthe crude product was purified
7. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)